HRID1277814
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
146 mg of phenyl isocyanate was added to a solution of 186 mg (1.2 mmol) of methyl 4-aminopicolate in 4 ml of dry acetone. The resulting mixture was agitated at room temperature overnight. Solvent was then evaporated off and the residue chromatographed in a conventional manner using silica gel (solvent:CHCl3 :acetone=4:1 volume). Fractions were collected and solvent removed by distillation. The residue was recrystallized from methanol to give the desired product having a melting point of 206°-208° C. (decompd.) in an amount of 261 mg (yiled 78.6%).
WORKUP
后处理
- customSolvent was then evaporated off
- customthe residue chromatographed in a conventional manner
- customFractions were collected
- customsolvent removed by distillation
- customThe residue was recrystallized from methanol